Laboratory continuous feeding negative pressure desolventizing device

Abstract

The utility model relates to the technical field of laboratory negative pressure desolventizing devices, in particular to a laboratory continuous feeding negative pressure desolventizing device which comprises a glass desolventizing kettle, the top end of the glass desolventizing kettle is connected with a straight condensation pipe, one end of the straight condensation pipe inclines downwards and is connected with a solvent receiving intermediate tank through a bent pipe distillation head, and the other end of the straight condensation pipe is connected with a vacuum pump. An intermediate tank bottom valve is arranged at the bottom end of the solvent receiving intermediate tank, a balance pipe is connected to the bottom end of the intermediate tank bottom valve, and a solvent bottle is connected to the bottom end of the balance pipe. According to the continuous feeding negative-pressure desolventizing device for the laboratory, the separation of boiling-point substances and high-boiling-point substances is greatly reduced under the vacuum degrees of different steps, and the residue of low-boiling-point substances in the high-boiling-point substances is lower than 50PPm; the continuous feeding can save the desolventizing time and improve the separation efficiency, the operation is simple, the solvent recovery adopts isolated receiving without stopping a vacuum system, the energy consumption of heating equipment is reduced, the health of experimenters is protected, and the working environment is protected.

Description

Technical Field

[0001] The utility model relates to the technical field of laboratory negative pressure desolventizing devices, in particular to a laboratory continuous feeding negative pressure desolventizing device. Background Art

[0002] For the point separation of low-boiling point substances (n-heptane, cyclohexane, toluene, ethyl acetate, methanol, ethanol, etc.) and high-boiling point substances (acrylates, methacrylate polyols, acids, etc.) in the laboratory, the volume of the experimental glass desolventizing kettle is limited, and it is impossible to load all the solvents and materials at once, and intermittent feeding is required.

[0003] Traditional laboratory negative pressure devices have low pressure gradients and lack pressure steps, making them unable to guarantee the removal of residual low-boiling-point substances. Intermittent feeding requires cooling the glass desolventizer and then heating it up after adding the material. This method is inefficient, cumbersome, unsafe, environmentally unfriendly, and consumes a lot of energy for heating equipment. To address these issues, we propose a laboratory continuous-feed negative pressure desolventizer. Utility Model Content

[0004] The purpose of the embodiment of the utility model is to provide a laboratory continuous feeding negative pressure desolventizing device, which solves the problems in the background technology.

[0005] To achieve the above objectives, the present invention provides the following technical solutions:

[0006] A laboratory continuous feeding negative pressure desolventizing device comprises a glass desolventizing kettle, the top of which is connected to a straight condenser, one end of which is inclined downward and is connected to a solvent receiving intermediate tank via a curved distillation head, the bottom end of which is provided with an intermediate tank bottom valve, the bottom end of which is connected to a balance pipe, and the bottom end of which is connected to a solvent bottle;

[0007] The top of the balance pipe is connected to a long tube, the bottom of the long tube is connected to a buffer bottle, the top of the buffer bottle is connected to a short tube, and the top of the short tube is connected to a desolventizing recovery system and a tail gas absorption system through a tee pipe.

[0008] Preferably, the desolventizing and recovery system comprises a water ring pump exhaust pipe, one end of the water ring pump exhaust pipe away from the tee pipe is connected to a water ring vacuum pump, and a water ring pump exhaust valve is provided on the water ring pump exhaust pipe.

[0009] Preferably, the exhaust gas absorption system includes a Roots pump exhaust pipe, one end of the Roots pump exhaust pipe away from the tee is connected to a Roots vacuum pump, and a Roots pump exhaust valve is provided on the Roots pump exhaust pipe.

[0010] Preferably, it also includes a finished product feeding tank, a finished product tank feeding valve is provided at the bottom of the finished product feeding tank, one end of the finished product tank feeding valve is connected to the desolventizing kettle feeding valve, and the desolventizing kettle feeding valve is connected to the glass desolventizing kettle at one end away from the desolventizing tank feeding valve.

[0011] Preferably, the glass desolventizing kettle is connected to an air inlet pipe of the desolventizing kettle;

[0012] A heating jacket is provided outside the glass desolventizing kettle, and an in-kettle thermometer is provided inside the glass desolventizing kettle.

[0013] Preferably, the top of the glass desolventizing kettle is connected to a straight condenser through a three-way distillation head, and a gas phase thermometer is inserted into one end of the three-way distillation head.

[0014] Preferably, an intermediate tank bottom valve is provided between the balancing pipe and the solvent receiving intermediate tank, and a vent valve is connected to the top of the solvent bottle.

[0015] Preferably, a first vacuum valve is provided on the balance pipe, and a second vacuum valve is provided on the long pipe;

[0016] One end of the long tube away from the buffer bottle is connected to the elbow distillation head.

[0017] Preferably, it further comprises a low-temperature circulating water pump, one end of which is connected to the cooling water inlet of the straight condenser tube via an upper water pipe, and the other end of which is connected to the cooling water outlet of the straight condenser tube via a return water pipe;

[0018] The return water pipe is provided with a return water valve, and the supply water pipe is provided with a supply water valve.

[0019] Preferably, the solvent receiving intermediate tank and the buffer bottle are connected to the return pipe through pipelines respectively, and the solvent receiving intermediate tank and the buffer bottle are connected to the water supply pipe through pipelines respectively.

[0020] By means of the above technical solution, the present invention provides a laboratory continuous feeding negative pressure desolventizing device. It has at least the following beneficial effects:

[0021] (1) The laboratory's continuous feeding negative pressure desolventizing device can greatly reduce the separation of boiling point substances and high boiling point substances under different levels of vacuum. The low boiling point substance remains below 50PPm in the high boiling point substance. Continuous feeding can save desolventizing time, improve separation efficiency, and is simple to operate. Solvent recovery uses isolated receiving without stopping the vacuum system, reducing the energy consumption of heating equipment, and is good for the health of experimental personnel and the environment.

[0022] (2) the laboratory continuous feeding negative pressure desolventizing device, the glass desolventizing kettle is fed through the product tank feed valve control glass desolventizing kettle feed flow, through the heating jacket control desolventizing kettle temperature, low boiling point gasification temperature, pressure, realize continuous desolventizing, gradient improve negative pressure is beneficial to low boiling point material separation, low boiling point material isolation collection and continuous heating save time and reduce power consumption, glass jacket design improves the recovery rate of low boiling point material, continuous feeding improves the desolventizing efficiency, simple operation, not friendly to the working environment, simple operation, safe and reliable purpose. BRIEF DESCRIPTION OF DRAWINGS

[0023] The drawings described herein are used to provide further understanding of the present application and form a part of the present application.

[0024] Figure 1 It is the overall structure schematic diagram of the embodiment of the present application.

[0025] In the figure: 1, feed product tank; 2, product agitator; 3, product tank emptying valve; 4, product tank feed valve; 5, display module; 6, desolventizing agitator; 7, gas phase thermometer; 8, with silk port sleeve; 9, desolventizing kettle feed valve; 10, kettle thermometer; 11, desolventizing kettle gas inlet pipe; 12, glass desolventizing kettle; 13, heating jacket; 14, balance pipe; 15, desolventizing kettle feed pipe; 16, straight type condenser pipe; 17, three-way distillation head; 18, low temperature circulating water pump; 19, backwater valve; 20, water inlet valve; 21, elbow distillation head; 22, solvent receiving intermediate tank; 23, intermediate tank bottom valve; 24, sleeve plug; 25, solvent bottle; 26, first vacuum valve; 27, second vacuum valve; 28, long pipe; 29, short pipe; 30, buffer bottle; 31, water ring pump air extraction valve; 32, Roots pump air extraction valve; 33, Roots vacuum pump; 34, water ring vacuum pump; 35, water ring pump water outlet valve; 36, feeding valve; 37, feeding hopper; 38, vent valve; 39, Roots pump air extraction pipe; 40, water ring pump air extraction pipe; 41, backwater pipe; 42, water inlet pipe. DETAILED DESCRIPTION

[0026] The technical scheme in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor belong to the scope of protection of the present application.

[0027] Please refer to Figure 1 The present application provides a technical scheme:

[0028] A laboratory continuous feeding negative pressure desolventizing device includes a finished product feeding tank 1, which is in a negative pressure state and is equipped with a hot water inlet and a hot water outlet. The finished product feeding tank 1 is equipped with an insulation jacket to provide thermal insulation according to experimental requirements. A finished product agitator 2 is located within the finished product feeding tank 1, and a feeding funnel 37 is located at the top of the finished product feeding tank 1, which is equipped with a feeding valve 36.

[0029] As a preferred embodiment, a finished product tank drain valve 3 and a finished product tank feed valve 4 are provided at the bottom of the finished product tank 1. The finished product tank feed valve 4 is connected to the desolventizing kettle feed valve 9 via the desolventizing kettle feed pipe 15. The desolventizing kettle feed pipe 15 is a silicone vacuum tube. The end of the desolventizing kettle feed valve 9 away from the desolventizing kettle feed pipe 15 is connected to the glass desolventizing kettle 12. The feed flow rate is controlled by the finished product tank feed valve 4 and the desolventizing kettle feed valve 9 under low negative pressure.

[0030] The glass desolventizing vessel 12 is connected to an air inlet pipe 11 for introducing nitrogen or air into the vessel for desolventizing. A variable frequency agitator 6 is provided within the vessel, which can adjust the speed. A thermometer 10 is also provided within the vessel for monitoring the temperature within the vessel. A heating jacket 13 is provided outside the vessel to control the temperature within the vessel, separating low-boiling-point substances from high-boiling-point substances. A lifting platform is provided at the bottom of the heating jacket 13 for adjusting the height of the vessel 12.

[0031] In a preferred embodiment, a three-way still 17 is connected to the top of the glass desolventizing kettle 12. A threaded sleeve 8 is provided at one end of the still 17. A vapor-phase thermometer 7 is inserted into the threaded sleeve 8 to continuously monitor the temperature changes of low-boiling-point substances. Both the kettle thermometer 10 and the vapor-phase thermometer 7 are electrically connected to a display module 5 for displaying the temperature.

[0032] One end of the three-way distillation head 17 is connected to a straight condenser 16. The straight condenser 16 comprises an inner tube and an outer tube. The outer tube is sleeved over the inner tube and is provided with a cooling water inlet and a cooling water outlet. In this embodiment, the cooling water is ice water. Both ends of the inner tube pass through the outer tube and are provided with connection ports.

[0033] The end of the inner tube of the straight condenser 16 away from the three-way distillation head 17 is tilted downward and connected to the solvent receiving intermediate tank 22 through the elbow distillation head 21. The solvent receiving intermediate tank 22 is provided with an insulation jacket, which can keep solvents with different freezing points warm or cold.

[0034] In a preferred embodiment, the bottom end of the solvent receiving intermediate tank 22 is provided with an intermediate tank bottom valve 23, the bottom end of the intermediate tank bottom valve 23 is connected to the balancing pipe 14, the bottom end of the balancing pipe 14 is connected to the solvent bottle 25, and the top of the solvent bottle 25 is connected to the vent valve 38. The top end of the solvent bottle 25 is provided with a cannula plug 24, and the balancing pipe 14 is inserted into the cannula plug 24.

[0035] A long tube 28 is connected to the elbow distillation head 21 , and the top of the balancing tube 14 is connected to the long tube 28 . A first vacuum valve 26 is provided on the balancing tube 14 , and a second vacuum valve 27 is provided on the long tube 28 .

[0036] The bottom end of the long tube 28 is connected to a buffer bottle 30 , and the top end of the buffer bottle 30 is connected to a short tube 29 .

[0037] The top end of the short tube 29 is connected to a Roots pump exhaust pipe 39 and a water ring pump exhaust pipe 40 through a tee. The end of the Roots pump exhaust pipe 39, away from the tee, is connected to a Roots vacuum pump 33, which is used to separate residual solvent. A Roots pump exhaust valve 32 is provided on the Roots pump exhaust pipe 39. The end of the water ring pump exhaust pipe 40, away from the tee, is connected to a water ring vacuum pump 34. A water ring pump exhaust valve 31 is provided on the water ring pump exhaust pipe 40. One end of the water ring vacuum pump 34 is connected to a water ring pump outlet valve 35.

[0038] The water ring pump exhaust pipe 40, water ring vacuum pump 34, water ring pump exhaust valve 31, and water ring pump outlet valve 35 constitute a solvent removal and recovery system to recover the solvent. The Roots pump exhaust pipe 39, Roots vacuum pump 33, and Roots pump exhaust valve 32 constitute an exhaust gas recovery system to prevent exhaust gas from remaining.

[0039] The cooling water outlet on the outer tube of the straight condenser 16 is connected to the low-temperature circulating water pump 18 through a return pipe 41, and a return valve 19 is provided on the return pipe 41. The cooling water inlet on the outer tube of the straight condenser 16 is connected to the low-temperature circulating water pump 18 through a water supply pipe 42, and a water supply valve 20 is provided on the water supply pipe 42.

[0040] The solvent receiving intermediate tank 22 and the buffer bottle 30 are connected to the return pipe 41 through pipelines. The solvent receiving intermediate tank 22 and the buffer bottle 30 are connected to the water supply pipe 42 through pipelines.

[0041] Working principle: when the glass desolventizing kettle 12 is in a negative pressure state, open the finished product tank feeding valve 4 and the desolventizing kettle feeding valve 9, and the material is sucked into the glass desolventizing kettle 12 through negative pressure, and the temperature in the kettle is controlled through the heating jacket 13 to separate the low-boiling-point substance from the high-boiling-point substance. The glass desolventizing kettle 12 is in a low negative pressure state, and the material enters 1 / 3 of the liquid level, the stirring is set, the heating temperature is set, and N2 or air is introduced for desolventizing. The low-boiling-point substance enters the straight condenser tube 16 under a certain negative pressure after the temperature is detected by the desolventizing kettle gas phase thermometer 7, and the shell side is ice water. The low-boiling-point substance enters the solvent receiving intermediate tank 22 through the straight condenser tube 16, and when the liquid level of the solvent receiving intermediate tank 22 reaches 80%, the intermediate tank bottom valve 23 is opened, and the solvent or low-boiling-point substance is put into the solvent bottle 25. When the liquid level of the solvent bottle 25 is 80%, the intermediate tank bottom valve 23 and the first vacuum valve 26 are closed, and the solution in the solvent bottle 25 is recovered, which can realize continuous feeding and desolventizing.

[0042] The jacket buffer bottle 30, the water ring pump air extraction valve 31, the water ring vacuum pump 34 and the Roots vacuum pump 33 are connected with the distillation head through silica gel vacuum pipes at one end and connected with the jacket buffer bottle 30 at the other end. The ice water is introduced into the buffer bottle jacket 30 to further cool and recover the low-boiling-point substance. The short pipe 29 is connected with the water ring pump air extraction valve 31 and the Roots pump air extraction valve 32 through the vacuum silica gel pipe. In the feeding stage, the Roots pump air extraction valve 32 and the Roots vacuum pump 33 are closed, and the water ring pump air extraction valve 31 and the water ring vacuum pump 34 are opened,

[0043] In the late desolventizing stage, when the residual amount of the solvent or low-boiling-point substance in the glass desolventizing kettle 12 is lower than 10000PPm according to the kettle thermometer 10, the gas phase thermometer 7 and the water ring vacuum pump 34, the Roots vacuum pump 33 and the Roots pump air extraction valve 32 are opened, and the water ring pump air extraction valve 31 and the water ring vacuum pump 34 are closed. The residual solvent is separated under the pressure of the Roots pump 1Pa-10Pa, which can realize that the conversion time from low negative pressure to high negative pressure can be continuously and alternately performed, and the Roots vacuum pump 33, the water ring vacuum pump 34, the waste liquid and the waste gas enter the absorption recovery system, and the whole system does not need to be stopped to switch the pump, which realizes simple operation, continuous feeding, high efficiency, environmental protection and safety. The Roots pump high negative pressure separates the low-boiling-point substance to solve the problem of residual low-boiling-point substance, and only the valve needs to be controlled, which is simple to operate. The Roots pump tail gas and the water ring vacuum pump 34 waste water enter the recovery system, and the solvent bottle 25 is emptied to enter the recovery system, which is friendly to the environment.

[0044] It should be noted that, in this document, relational terms such as first and second, etc., are used only to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the terms "comprises," "comprising," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that includes a list of elements includes not only those elements but also other elements not explicitly listed, or elements inherent to such process, method, article, or apparatus.

[0045] Although the embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the present invention, and the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A laboratory continuous feeding negative pressure desolventizing device, comprising a glass desolventizing kettle (12), characterized in that: The top of the glass desolventizing kettle (12) is connected to a straight condenser (16), one end of the straight condenser (16) is tilted downward and is connected to a solvent receiving intermediate tank (22) through a curved distillation head (21), the bottom end of the solvent receiving intermediate tank (22) is provided with an intermediate tank bottom valve (23), the bottom end of the intermediate tank bottom valve (23) is connected to a balance pipe (14), and the bottom end of the balance pipe (14) is connected to a solvent bottle (25); The top end of the balancing pipe (14) is connected to a long pipe (28), the bottom end of the long pipe (28) is connected to a buffer bottle (30), the top end of the buffer bottle (30) is connected to a short pipe (29), and the top end of the short pipe (29) is respectively connected to a desolventizing recovery system and a tail gas absorption system through a three-way pipe.

2. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The desolventizing and recovery system comprises a water ring pump exhaust pipe (40), one end of the water ring pump exhaust pipe (40) away from the tee pipe is connected to a water ring vacuum pump (34), and a water ring pump exhaust valve (31) is provided on the water ring pump exhaust pipe (40).

3. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The tail gas absorption system comprises a Roots pump exhaust pipe (39), one end of the Roots pump exhaust pipe (39) away from the tee is connected to a Roots vacuum pump (33), and a Roots pump exhaust valve (32) is provided on the Roots pump exhaust pipe (39).

4. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The invention also comprises a finished product feeding tank (1), wherein a finished product tank feeding valve (4) is provided at the bottom of the finished product feeding tank (1), one end of the finished product tank feeding valve (4) is connected to a desolventizing kettle feeding valve (9), and the end of the desolventizing kettle feeding valve (9) away from the desolventizing tank feeding valve (4) is connected to a glass desolventizing kettle (12).

5. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The glass desolventizing kettle (12) is connected to a desolventizing kettle air inlet pipe (11); A heating jacket (13) is provided outside the glass desolventizing kettle (12), and an in-kettle thermometer (10) is provided inside the glass desolventizing kettle (12).

6. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The top of the glass desolventizing kettle (12) is connected to the straight condenser (16) through a three-way distillation head (17), and a gas phase thermometer (7) is inserted into one end of the three-way distillation head (17).

7. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: An intermediate tank bottom valve (23) is provided between the balance pipe (14) and the solvent receiving intermediate tank (22), and a vent valve (38) is connected to the top of the solvent bottle (25).

8. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The balance pipe (14) is provided with a first vacuum valve (26), and the long pipe (28) is provided with a second vacuum valve (27); One end of the long tube (28) away from the buffer bottle (30) is connected to the elbow distillation head (21).

9. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: It also includes a low-temperature circulating water pump (18), one end of which is connected to the cooling water inlet of the straight condenser tube (16) through an upper water pipe (42), and the other end of which is connected to the cooling water outlet of the straight condenser tube (16) through a return water pipe (41); The return water pipe (41) is provided with a return water valve (19), and the supply water pipe (42) is provided with a supply water valve (20).

10. The laboratory continuous feeding negative pressure desolventizing device according to claim 1, characterized in that: The solvent receiving intermediate tank (22) and the buffer bottle (30) are respectively connected to the return pipe (41) through pipelines, and the solvent receiving intermediate tank (22) and the buffer bottle (30) are respectively connected to the water supply pipe (42) through pipelines.

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